The methyl esters can be injected directly from the reaction solvents. A plasma volume of 50 μL was used without special purification. The detection limits were around 0.1 ng/μL. The proposed method avoids the drawbacks of the previous methods used for the one-step analysis of individual free fatty acids in human plasma.Lithium ion batteries are essential power sources in portable electronics, electric vehicles and as energy storage devices for renewable energies. During harsh battery cell operation as well as at elevated temperatures, the electrolyte decomposes and inter alia organo(fluoro)phosphates are formed due to hydrolysis of the conducting salt lithium hexafluorophosphate (LiPF6). Since these phosphorus-containing decomposition products possess a potential toxicity based on structural similarities compared to chemical warfare agents, quantification is of high interest regarding safety estimates. In this study, two comprehensive approaches for the precipitation of highly concentrated PF6¯ were investigated, allowing the separation from target analytes (organo(fluoro)phosphates) and improving mass spectrometry-based quantification techniques. Trimethyl phosphate was used as a polar, non-acidic organophosphate reference substance for method development via liquid chromatography-mass spectrometry. Six solvents were examined regarding precipitation reaction and selectivity. Thermally degraded electrolytes were analyzed after precipitation by means of gas chromatography-flame ionization detector, demonstrating the applicability of the developed sample preparations. The optimized method was applied successfully without influencing any volatile and non-acidic decomposition products. Using optimized conditions, a precipitation rate of 98% PF6¯ was achieved. Consequently, a fast and easy sample preparation for gas chromatographic investigations on lithium ion battery electrolytes was implemented, applicable for routine analysis.Novel Psychoactive Substances (NPS) represent an alternative to established illicit drugs. They are traded via the internet and exhibit small alterations in their chemical structure to circumvent law, however, their psychotropic effects are comparable. There is still poor knowledge about side effects and health risks. By the end of 2018, 730 NPS were reported to EMCDDA (European Monitoring Centre for Drugs and Drug Addiction). Among different compound classes, many NPS are chiral and few publications deal with the different pharmacological and toxicological properties of their pure enantiomers. Therefore, analytical method development concerning enantioseparation of NPS is of great interest. Chiral separation protocols of established illicit drugs have been transferred for NPS, selected examples are given as well. Different methods for enantioseparation of NPS comprising mainly stimulating drugs such as cathinones, pyrovalerones, amphetamines, ketamines, (2-aminopropyl) benzofuranes, phenidines, phenidates, morpholines and thiophenes are reviewed. Moreover, chiral resolution of some cannabinomimetics by HPLC is presented. Chromatographic and electrophoretic techniques such as GC, HPLC, SFC, CE and CEC are discussed and in some cases compared. Mainly, solid samples either purchased from internet vendors, seized by police or collected from patients in hospitals are subject to analysis. Chiral selectors used for HPLC are listed in a Table. It was shown that particularly stimulating drugs are traded as racemic mixtures, which is not the case with cannabinomimetics. Mainly, HPLC and CE were used for enantioseparation of NPS.Analysis and control of stereoisomers is a major task in pharmaceutical analysis, and is a greater challenge when compounds with multiple chiral centers (MCC) are concerned. HPLC and SFC are commonly used for stereoisomer analysis in drug development, typically starting with chiral method screening. Although method screening for compounds with a single chiral center (SCC) has been well studied for 5-?m polysaccharide stationary phase particles, there are fewer reports on method screening for compounds with MCC and smaller particle sizes. In this study, we systematically evaluated the impact of key parameters in chiral method screening including column particle size (3-?m vs. sub-2 ?m), nature of the chiral selector binding (coated vs. immobilized), mobile phase elution mode (isocratic vs. gradient), and separation approach (SFC vs. https://www.selleckchem.com/products/cl-amidine.html HPLC). A diverse set of pharmaceutical compounds with MCC and a SCC were studied. We found that the screening strategies differ between MCC and SCC compounds due to the difference in the recognition mechanism involved. Furthermore, we have developed an effective screening strategy with OD-3, AD-3 and IG-3 columns for SCC compounds which achieves larger than 90% success rate, and a combination of OD-3, AD-3, IG-3, IC-3 and AS-3 for MCC compounds which offers the best coverage.Natural estrogens (estrone E1, 17β-estradiol E2, estriol E3) and the synthetic estrogen (17α-ethinylestradiol EE2) are endocrine disruptors harmful to aquatic wildlife. The European Commission included these molecules in the surface water Watch Lists issued in 2015 and 2018 under the Water Framework Directive regarding emerging aquatic pollutants, proposing maximum detection limits (LOD) of 0.035 ng/L for EE2 and 0.4 ng/L for E1 and E2. Attaining these limits represents a challenge even with the most up-to-date analytical tools, in particular in surface water. A two-step sample preparation, involving a preliminary extraction of a whole water sample on a solid-phase extraction (SPE) disk and further purification on a Florisil SPE cartridge, was optimized. The purified extract was derivatized subsequently and quantified by LC-MS/MS. The main goal was to maximize the recoveries to achieve the very low LODs required by the European Watch Lists. The method was fully validated in seven surface water. The LODs calculated were below the maximum acceptable limits required by the European Commission.Synthetic opioids are responsible for numerous overdoses and fatalities worldwide. Currently, fentanyl and its analogs are also mixed with heroin, cocaine and methamphetamine, or sold as oxycodone, hydrocodone and alprazolam in counterfeit medications. Microextraction techniques became more frequent in analytical toxicology over the last decade. A method to simultaneously quantify nine synthetic opioids, fentanyl, sufentanil, alfentanil, acrylfentanyl, thiofentanyl, valerylfentanyl, furanylfentanyl, acetyl fentanyl and carfentanil, and two metabolites, norfentanyl and acetyl norfentanyl, in urine samples by microextraction with packed sorbent (MEPS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and validated. A multivariate optimization was performed to establish the number and speed (stroke) of draw-eject sample cycles and the extraction solvent. The best extraction condition was eight draw-eject sample cycles, with a velocity of 3.6 ?L/sec and acetonitrile as elution solvent. Linearity was achieved between 1 to 100 ng/mL, with a limit of detection (LOD) of 0.